Hydrogen Peroxide → HCID 14404512, compound

HRID 2106836Notes

Reaction equation

HRID 2106836 reaction equation
[CH2:1]([S:8][CH2:9][CH2:10][CH2:11][Cl:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH:13]O>C(O)(=O)C.O>[CH2:1]([S:8]([CH2:9][CH2:10][CH2:11][Cl:12])=[O:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

5

Procedure

1.2 g of 1-benzylthio-3-chloro-n-propane, synthesized by ◯1 of Synthesis Example 2 was dissolved in 50 ml of acetic acid, and 8.7 g of 35% aqueous hydrogen peroxide was added thereto dropwise under stirring below 10° C. After that, it was warmed gradually to room temperature again, then stirred further for 4 hours. The reaction mixture was poured in 300 ml of iced water, and extracted 2 times by each 150 ml of methylene chloride. The methylene chloride layer was washed 2 times with 5% aqueous solution of sodium hydroxide, followed by water, and dried over anhydrous magnesium sulfate. A colorless solid residue was obtained by distilling off methylene chloride. It was washed by n-hexane to give 12.6 g (yield: 96.9%) of the object 1-benzylsulfinyl-3-chloro-n-propane as a colorless crystal. m.p. 70° to 71° C.

Workup

  1. stirringstirred further for 4 hours
  2. extractionextracted 2 times by each 150 ml of methylene chloride
  3. washThe methylene chloride layer was washed 2 times with 5% aqueous solution of sodium hydroxide
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customA colorless solid residue was obtained
  6. distillationby distilling off methylene chloride
  7. washIt was washed by n-hexane

Sources & evidence

ORD record
ord-1082503d5b4841d3bc51b34d348d45fb
Source dataset
uspto-grants-1990_06
Patent number
US04931474

Reaction notes

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